HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 136052978, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 136052980 | HCID 136052980 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 136052978 | HCID 136052978 | — |
Reaction Steps
95 mg (0.162 mmol) of 2-{4-[7-({[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methyl}sulfanyl)-6-cyano-2-methyl-4-oxo-3,4-dihydropyrido[2,3-d]pyrimidin-5-yl]phenoxy}ethyl acetate were initially charged in 10 ml of a dioxane/water mixture 2:1, 7.7 mg (0.323 mmol) of lithium hydroxide were added and the mixture was stirred at RT for 5 h. The reaction mixture was then diluted with water, acidified with 1N hydrochloric acid and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, the drying agent was filtered off and the filtrate was concentrated. The residue was purified by preparative HPLC (mobile phase gradient: acetonitrile/water 10:90→95:5, with 0.1% TFA added). This gave 88 mg (99% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618119B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-657be9311f254c579643dfc80aafc1f9 |
| Source note | uspto-grants-2013_12 |